Preparo e caracterização de material de referência de solo para nutrientes e contaminantes inorgânicos
Autor(a) principal: | |
---|---|
Data de Publicação: | 2014 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFSCAR |
Texto Completo: | https://repositorio.ufscar.br/handle/ufscar/6600 |
Resumo: | The certified reference materials make an important role in the establishment of traceability in analytical chemistry, ensuring reliability and accuracy to the measurements and are fundamental for the validation of analytical methods. The demand for new certified reference materials increases in all areas of knowledge, with emphases to the agriculture. Basis for the production of farming products, the demand for soil analysis is great and the existence of a reference material of a typical Brazilian soil is important to ensure the quality of results. In this context, the present work describe the preparate and the characterization of a national reference material for Cr, Pb, Cd, and As soil contaminants and Ca, P, Mg, K, Cu, Fe, Mn, Zn, and Na macro and micronutrients. The material was produced following the internationally accepted ISO Guides 30-35 norms considering the preparation and packaging, homogeneity, short and long term stability, and material characterization and certification. A Typic Paleudult soil was artificially contaminated with As, Cd, Cr, and Pb, added as salt solutions from Pb(NO3)2; Cd(NO3)2.4H2O; Na2HAsO4.7H2O, and Cr(NO3)3.9H2O salts. After 12 month of contamination, 65 kg of soil was dried at room temperature, ground (particles size < 390μm), homogenized, packaged and irradiated with gamma ray (20 - 25 kGy) aiming to increase the shelf-life. The analyte soil extractions were based on methodology recommended by Brazilian legislation (CONAMA N° 420), with in turn follows the protocol established by American environmental agency (USEPA 3051). It was performed by assisted microwave oven with the use of 14 mol L-1 HNO3. The evaluation of the estimate minimum amount, homogeneity and stability of the material were carried out, using inductively coupled plasma optical emission spectroscopy (ICP OES) determination technique. The results were submitted to analysis of variance of single factor (ANOVA). The homogeneity and stability of the material presented means within a confidence interval of 95% for As, Cd, Pb, Cr, Ca, Cu, Fe, Na, K, Mg, Mn, and P. The chemical characterization of the material was performed through a collaborative test and the uncertainties related to each step of the material prepare were calculated to obtain the expanded uncertainty for each one of the analytes and to the final drafting of the control chart with the results of the reference material. |
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Verhalen, Tatiane RosaneNogueira, Ana Rita de Araújohttp://lattes.cnpq.br/7034773971317045http://lattes.cnpq.br/6996574853570916959597ca-a15d-4624-8905-b2a210f04a502016-06-02T20:36:53Z2014-11-132016-06-02T20:36:53Z2014-09-26VERHALEN, Tatiane Rosane. Prepare and characterization of a soil reference material for inorganic nutrients and contaminants. 2014. 124 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2014.https://repositorio.ufscar.br/handle/ufscar/6600The certified reference materials make an important role in the establishment of traceability in analytical chemistry, ensuring reliability and accuracy to the measurements and are fundamental for the validation of analytical methods. The demand for new certified reference materials increases in all areas of knowledge, with emphases to the agriculture. Basis for the production of farming products, the demand for soil analysis is great and the existence of a reference material of a typical Brazilian soil is important to ensure the quality of results. In this context, the present work describe the preparate and the characterization of a national reference material for Cr, Pb, Cd, and As soil contaminants and Ca, P, Mg, K, Cu, Fe, Mn, Zn, and Na macro and micronutrients. The material was produced following the internationally accepted ISO Guides 30-35 norms considering the preparation and packaging, homogeneity, short and long term stability, and material characterization and certification. A Typic Paleudult soil was artificially contaminated with As, Cd, Cr, and Pb, added as salt solutions from Pb(NO3)2; Cd(NO3)2.4H2O; Na2HAsO4.7H2O, and Cr(NO3)3.9H2O salts. After 12 month of contamination, 65 kg of soil was dried at room temperature, ground (particles size < 390μm), homogenized, packaged and irradiated with gamma ray (20 - 25 kGy) aiming to increase the shelf-life. The analyte soil extractions were based on methodology recommended by Brazilian legislation (CONAMA N° 420), with in turn follows the protocol established by American environmental agency (USEPA 3051). It was performed by assisted microwave oven with the use of 14 mol L-1 HNO3. The evaluation of the estimate minimum amount, homogeneity and stability of the material were carried out, using inductively coupled plasma optical emission spectroscopy (ICP OES) determination technique. The results were submitted to analysis of variance of single factor (ANOVA). The homogeneity and stability of the material presented means within a confidence interval of 95% for As, Cd, Pb, Cr, Ca, Cu, Fe, Na, K, Mg, Mn, and P. The chemical characterization of the material was performed through a collaborative test and the uncertainties related to each step of the material prepare were calculated to obtain the expanded uncertainty for each one of the analytes and to the final drafting of the control chart with the results of the reference material.Os materiais de referência certificados desempenham papel fundamental no estabelecimento da rastreabilidade em química analítica, assegurando confiabilidade e exatidão dos resultados de medição e são fundamentais para a validação dos métodos analíticos. A demanda por novos materiais de referência cresce a cada dia, em todas as áreas do conhecimento, entre as quais destaca-se a agricultura. Base para a produção dos produtos agrícolas, a demanda por análises de solo é grande e a existência de um material de referência de solo tipicamente brasileiro é importante para garantir a qualidade dos resultados. Nesse contexto, o presente trabalho descreve o preparo e a caracterização de um material de referência nacional de solo para os contaminantes Cr, Pb, Cd e As e os macro e micronutrientes Ca, P, Mg, K, Cu, Fe, Mn, Zn e Na. O material foi produzido seguindo as etapas, estabelecidas pelas normas ISO GUIAS 30 a 35, internacionalmente aceitas no preparo e envase do material, na avaliação da homogeneidade, no teste de estabilidade a curto e a longo períodos e na certificação do material. O solo utilizado, latossolo vermelho amarelo foi artificialmente contaminado com Cr, Pb, Cd e As, adicionados na forma de soluções preparadas a partir dos seguintes sais: Pb(NO3)2; Cd(NO3)2.4H2O; Na2HAsO4.7H2O e Cr(NO3)3.9H2O. Após 12 meses da adição dos contaminantes, 65 kg de solo foi seco a temperatura ambiente, moído (granulometria < 390 μm), homogeneizado, envasado e irradiado com radiação gama (20 - 25 kGy), visando o aumento do tempo de prateleira. O preparo da amostra visando obtenção dos teores extraíveis dos analitos empregou ácido nítrico 14 mol L-1 com aquecimento assistido por radiação micro-ondas e foi baseada em metodologia recomendada pela legislação brasileira (CONAMA N° 420), que por sua vez segue protocolo estabelecido pelo órgão ambiental americano (USEPA 3051). A avaliação da estimativa da massa mínima, da homogeneidade e da estabilidade do material foi realizada utilizando-se como técnica de determinação a espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES). Os resultados foram submetidos à análise de variância de fator único (ANOVA). A homogeneidade e a estabilidade do material apresentaram médias dentro do intervalo de confiança de 95% para As, Cd, Pb, Cr, Ca, Cu, Fe, Na, K, Mg, Mn e P do material candidato a material de referência de solo. A caracterização química do material foi realizada por meio do ensaio colaborativo, com a participação de laboratórios nacionais e as incertezas associadas a cada passo da preparação do material foram calculadas para se obter a incerteza expandida para cada analito em estudo e a elaboração final da carta de controle com os resultados do material de referência.Financiadora de Estudos e Projetosapplication/pdfporUniversidade Federal de São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarBRQuímica analíticaMaterial de referênciaSolosICP-OESCIENCIAS EXATAS E DA TERRA::QUIMICAPreparo e caracterização de material de referência de solo para nutrientes e contaminantes inorgânicosPrepare and characterization of a soil reference material for inorganic nutrients and contaminantsinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesis-1-1e83fd9a0-c0d6-4518-b677-9aa885aeffbcinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINAL6310.pdfapplication/pdf1827814https://repositorio.ufscar.br/bitstream/ufscar/6600/1/6310.pdfb94dcad55360a35c44e4718db7d6fcacMD51TEXT6310.pdf.txt6310.pdf.txtExtracted texttext/plain0https://repositorio.ufscar.br/bitstream/ufscar/6600/4/6310.pdf.txtd41d8cd98f00b204e9800998ecf8427eMD54THUMBNAIL6310.pdf.jpg6310.pdf.jpgIM Thumbnailimage/jpeg9671https://repositorio.ufscar.br/bitstream/ufscar/6600/5/6310.pdf.jpg54f2b5ba56443b2a77f023369a744869MD55ufscar/66002023-09-18 18:30:40.437oai:repositorio.ufscar.br:ufscar/6600Repositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestopendoar:43222023-09-18T18:30:40Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false |
dc.title.por.fl_str_mv |
Preparo e caracterização de material de referência de solo para nutrientes e contaminantes inorgânicos |
dc.title.alternative.eng.fl_str_mv |
Prepare and characterization of a soil reference material for inorganic nutrients and contaminants |
title |
Preparo e caracterização de material de referência de solo para nutrientes e contaminantes inorgânicos |
spellingShingle |
Preparo e caracterização de material de referência de solo para nutrientes e contaminantes inorgânicos Verhalen, Tatiane Rosane Química analítica Material de referência Solos ICP-OES CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Preparo e caracterização de material de referência de solo para nutrientes e contaminantes inorgânicos |
title_full |
Preparo e caracterização de material de referência de solo para nutrientes e contaminantes inorgânicos |
title_fullStr |
Preparo e caracterização de material de referência de solo para nutrientes e contaminantes inorgânicos |
title_full_unstemmed |
Preparo e caracterização de material de referência de solo para nutrientes e contaminantes inorgânicos |
title_sort |
Preparo e caracterização de material de referência de solo para nutrientes e contaminantes inorgânicos |
author |
Verhalen, Tatiane Rosane |
author_facet |
Verhalen, Tatiane Rosane |
author_role |
author |
dc.contributor.authorlattes.por.fl_str_mv |
http://lattes.cnpq.br/6996574853570916 |
dc.contributor.author.fl_str_mv |
Verhalen, Tatiane Rosane |
dc.contributor.advisor1.fl_str_mv |
Nogueira, Ana Rita de Araújo |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/7034773971317045 |
dc.contributor.authorID.fl_str_mv |
959597ca-a15d-4624-8905-b2a210f04a50 |
contributor_str_mv |
Nogueira, Ana Rita de Araújo |
dc.subject.por.fl_str_mv |
Química analítica Material de referência Solos ICP-OES |
topic |
Química analítica Material de referência Solos ICP-OES CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The certified reference materials make an important role in the establishment of traceability in analytical chemistry, ensuring reliability and accuracy to the measurements and are fundamental for the validation of analytical methods. The demand for new certified reference materials increases in all areas of knowledge, with emphases to the agriculture. Basis for the production of farming products, the demand for soil analysis is great and the existence of a reference material of a typical Brazilian soil is important to ensure the quality of results. In this context, the present work describe the preparate and the characterization of a national reference material for Cr, Pb, Cd, and As soil contaminants and Ca, P, Mg, K, Cu, Fe, Mn, Zn, and Na macro and micronutrients. The material was produced following the internationally accepted ISO Guides 30-35 norms considering the preparation and packaging, homogeneity, short and long term stability, and material characterization and certification. A Typic Paleudult soil was artificially contaminated with As, Cd, Cr, and Pb, added as salt solutions from Pb(NO3)2; Cd(NO3)2.4H2O; Na2HAsO4.7H2O, and Cr(NO3)3.9H2O salts. After 12 month of contamination, 65 kg of soil was dried at room temperature, ground (particles size < 390μm), homogenized, packaged and irradiated with gamma ray (20 - 25 kGy) aiming to increase the shelf-life. The analyte soil extractions were based on methodology recommended by Brazilian legislation (CONAMA N° 420), with in turn follows the protocol established by American environmental agency (USEPA 3051). It was performed by assisted microwave oven with the use of 14 mol L-1 HNO3. The evaluation of the estimate minimum amount, homogeneity and stability of the material were carried out, using inductively coupled plasma optical emission spectroscopy (ICP OES) determination technique. The results were submitted to analysis of variance of single factor (ANOVA). The homogeneity and stability of the material presented means within a confidence interval of 95% for As, Cd, Pb, Cr, Ca, Cu, Fe, Na, K, Mg, Mn, and P. The chemical characterization of the material was performed through a collaborative test and the uncertainties related to each step of the material prepare were calculated to obtain the expanded uncertainty for each one of the analytes and to the final drafting of the control chart with the results of the reference material. |
publishDate |
2014 |
dc.date.available.fl_str_mv |
2014-11-13 2016-06-02T20:36:53Z |
dc.date.issued.fl_str_mv |
2014-09-26 |
dc.date.accessioned.fl_str_mv |
2016-06-02T20:36:53Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
VERHALEN, Tatiane Rosane. Prepare and characterization of a soil reference material for inorganic nutrients and contaminants. 2014. 124 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2014. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufscar.br/handle/ufscar/6600 |
identifier_str_mv |
VERHALEN, Tatiane Rosane. Prepare and characterization of a soil reference material for inorganic nutrients and contaminants. 2014. 124 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2014. |
url |
https://repositorio.ufscar.br/handle/ufscar/6600 |
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Universidade Federal de São Carlos |
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